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1.
A slurry sampling electrothermal atomic absorption spectrometry method for the determination of Al, Ca, Cd, Co, Cr, Cu, Fe, K, Li, Mg, Mn, Na, Ni, Pb, Sr, Tl and Zn in powdered titanium dioxide is described. The behaviour of the titanium matrix in the atomizer and its interferences with the determination of Al, Fe, Co, Ni and Mn were studied. A tungsten carbide modified graphite tube was used to improve the signal shape and the repeatability for the determination of Fe. For all elements, except for Cd and Pb, quantification by a calibration curve established with aqueous standards was possible. No chemical modifier was used throughout in order to minimize contamination. For the contamination risk elements such as Ca, Fe, K, Mg, Na and Zn, the slurry sampling technique allows to achieve limits of detection (3σ of the blank) 5–20 times lower than the solution technique, resulting for these elements in values of 1, 3, 0.5, 0.5, 0.9 and 2 ng g−1, respectively, and, generally being in the range of 0.2 ng g−1 (Cd) to 10 ng g−1 (Al and Tl). The results obtained by the slurry sampling technique are compared with those of other independent methods including four solution methods and neutron activation analysis.  相似文献   

2.
The Freundlich and Langmuir isotherms were used to describe the biosorption of Cu(II), Pb(II), and Zn(II) onto the saltbush leaves biomass at 297 K and pH 5.0. The correlation coefficients (R2) obtained from the Freundlich model were 0.9798, 0.9575, and 0.9963 for Cu, Pb, and Zn, respectively, while for the Langmuir model the R2 values for the same metals were 0.0001, 0.1380, and 0.0088, respectively. This suggests that saltbush leaves biomass sorbed the three metals following the Freundlich model (R2 > 0.9575). The KF values obtained from the Freundlich model (175.5 · 10−2, 10.5 · 10−2, and 6.32 · 10−2 mol · g−1 for Pb, Zn, and Cu, respectively), suggest that the metal binding affinity was in the order Pb > Zn > Cu. The experimental values of the maximal adsorption capacities of saltbush leaves biomass were 0.13 · 10−2, 0.05 · 10−2, and 0.107 · 10−2 mol · g−1 for Pb, Zn, and Cu, respectively. The negative ΔG values for Pb and the positive values for Cu and Zn indicate that the Pb biosorption by saltbush biomass was a spontaneous process.  相似文献   

3.
《Microchemical Journal》2011,97(2):380-385
Basic color data (RGB) obtained from digital images were studied by Factorial Analysis. The results demonstrated that individual RGB data represent different contributions. On the other hand, the total intensity of colors is proposed like a fourth variable in digital colorimetry and can be interpreted as complementary information related to the conditions of image capture in digital cameras. The chemometric study evidences that the analytical information, for quantitative applications, is formed by two parts: deterministic, with valuable analytical interest, and undeterministic or unvaluable analytical information. These results were revealed after variable reduction and data compression, using Principal Component Analysis and Fourier Transform, respectively.The digital colorimetric study was applied to the reaction of Ti(IV) with hydrogen peroxide at 0.09 M sulfuric acid media. They produce a yellow–orange complex solution. And their RGB intensities could be linearly correlated with Ti(IV) concentration in the range of 2.0 to 30.0 mg l 1. In the best conditions, using the intensity of the blue color, a simple and fast method for Ti(IV) determination could be developed. Its detection limit was found to be (criterion 3 s) 0.6 mg l 1 and the rsd for 10.0 mg l 1 of Ti(V) was 4.8%.Calibration by artificial neural nets represents an option that improves the answer to low concentration.Applications of the colorimetric method to the analysis of Ti in representative plastics, with content in mg g 1 level, are presented. Its validity was assessed by ICP-AES with standard addition. Results were in satisfactory agreement. The method is fast and reduces the analysis time.  相似文献   

4.
In this communication, we report the development of cobalt-sulfide nanosheets film on Ti mesh (Co-S/Ti mesh) via electrodeposition as a novel oxygen evolution anode in basic media. Electrochemical experiments suggest that this Co-S/Ti mesh electrode exhibits high catalytic activity and good stability. It needs overpotential of 361 mV to drive current density of 10 mA cm 2 and its catalytic activity is maintained for at least 20 h.  相似文献   

5.
《中国化学快报》2020,31(10):2752-2756
Electrochemical analysis is a promising technique for detecting biotoxic and non-biodegradable heavy metals. This article proposes a novel composite electrode based on a polyaniline (PANi) framework doped with bismuth nanoparticle@graphene oxide multi-walled carbon nanotubes (Bi NPs@GO-MWCNTs) for the simultaneous detection of multiple heavy metal ions. Composite electrodes are prepared on screen-printed electrodes (SPCEs) using an efficient dispensing technique. We used a SM200SX-3A dispenser to load a laboratory-specific ink with optimized viscosity and adhesion to draw a pattern on the work area. The SPCE was used as substrate to facilitate cost-effective and more convenient real-time detection technology. Electrochemical techniques, such as cyclic voltammetry and differential pulse voltammetry, were used to demonstrate the sensing capabilities of the proposed sensor. The sensitivity, limit of detection, and linear range of the PANi-Bi NPs@GO-MWCNT electrode are 2.57 × 102 μA L μmol−1 cm−2, 0.01 nmol/L, and 0.01 nmol/L–5 mmol/L and 0.15 × 10−1 μA L μmol−1 cm−2, 0.5 nmol/L, and 0.5 nmol/L–5 mmol/L for mercury ion (Hg(II)) and copper ion (Cu(II)) detection, respectively. In addition, the electrode exhibits a good selectivity and repeatability for Hg(II) and Cu(II) sensing when tested in a complex heavy metal ion solution. The constructed electrode system exhibits a detection performance superior to similar methods and also increases the types of heavy metal ions that can be detected. Therefore, the proposed device can be used as an efficient sensor for the detection of multiple heavy metal ions in complex environments.  相似文献   

6.
The advantages of using membrane micropumps rather than peristaltic pumps to introduce both sample and reagent solutions for hydride generation atomic fluorescence spectrometry are discussed. Arsenic was used as a test analyte to check the performance of the proposed manifold. Sample and reagent consumption was reduced 8–9 fold compared with continuous mode measurements made with peristaltic pumps, with no deterioration in sensitivity. The calibration graph was linear in the 0.05 to 2.5 μg l 1 As range using peak area as the analytical signal and maximum gain in the detector setting. A limit of detection (3σ) of 0.02 μg l 1 and relative standard deviation values close to 2% for 10 independent measurements of a 1 μg l 1 As solution were obtained. The sampling frequency increased from 45 to 102 h 1 with the subsequent saving in carrier gas used and reduction in wastes generated. The instrumental modification, which could be used for other elements currently determined by atomic fluorescence spectrometry, will permit hydride generators of more reduced dimensions to be constructed.  相似文献   

7.
《Microchemical Journal》2007,85(1-2):10-13
In this paper, a sensitive flow injection chemiluminescence system luminol–myoglobin was described for determining femtogram nitrite. Nitrite bound myoglobin producing the ferric heme nitrite complexes, which catalyzed the electron transfer of luminol to myoglobin leading to fast chemiluminescence. The chemiluminescence intensity in the presence of nitrite was remarkably enhanced compared with that in the absence of it. Under the optimum reaction conditions the chemiluminescence increment produced was proportional to the concentration of nitrite in the range of 0.05 pg ml 1–1.0 ng ml 1 (R2 = 0.9991), with a detection limit (3σ) of 20.0 fg ml 1. At the flow rate of 2.0 ml min 1, the whole process including sampling and washing could be completed in 0.5 min offering the sampling efficiency of 120 h 1 accordingly, and the relative standard deviation (RSD) was less than 2.60% (n = 5). It was satisfactory for the application to determine nitrite in human urine samples, and the possible mechanism was proposed.  相似文献   

8.
A flow injection on-line displacement solid-phase extraction protocol was employed to minimize mass interferences with determination of palladium by inductively coupled plasma mass spectrometry (ICP-MS). The developed method involved in on-line complexing of Ag+ with pyrrolidine dithiocarbamate (PDC), presorption of the resultant Ag–PDC onto a microcolumn packed with the cigarette filter, displacement sorption of Pd2+ through loading the sample solution onto the microcolumn due to on-line displacement reaction between Pd2+ and the presorbed Ag–PDC, elution of the retained Pd2+ with 50 μL of ethanol for on-line ICP-MS detection. Interferences from co-existing heavy metal ions with lower stability of their PDC complexes relative to Ag–PDC were minimized/eliminated. No interferences from 5 mg L 1 Zn and 3 mg L 1 Pb for 104Pd, 0.4 mg L 1 Cu for 105Pd, 6 mg L 1 Zn and 2 mg L 1 Cd for 106Pd, 6 mg L 1 Zn and 3 mg L 1 Cd for 108Pd, and 2 mg L 1 Cd for 110Pd were observed for the determination of 100 ng L 1 Pd. The enhancement factors of 71–75, sample throughput of 23 samples h 1 and detection limits of 2.8–3.5 ng L 1 were achieved with the consumption of 3.0 mL of sample solution. The precision (RSD) for eleven replicate determinations of Pd at the 100 ng L 1 level was 1.8–2.7%. The developed method was applied to the determination of palladium in rock samples.  相似文献   

9.
The paper presents the preconcentration of trace elements via electrodeposition onto a (micro)aluminum cathode in the presence of ionic liquid 1-butyl-3-methylimidazolium hexafluorophosphate [BMIM][PF6] as a supporting electrolyte. The advantages of the proposed method include very simple instrumentation for the preconcentration of trace elements and low-cost reagents. The experiment showed that the use of ionic liquid in the electrodeposition process significantly improves sensitivity, recovery and detection limits for the determination of trace amounts of iron, cobalt, nickel and zinc. The preconcentrated metals were determined using X-ray fluorescence spectrometry. The optimum parameters for electrodeposition such as pH, the volume of the analyzed solution, the voltage and the deposition time were studied. Under the optimized conditions, the detection limits were 5, 2, 3 and 6 μg L 1 for iron, cobalt, nickel and zinc, respectively. The precision and recovery of the method were in the range of 3–5.5%, and 92–103%, respectively. The calibration was performed using aqueous standards of Fe(III), Co(II), Ni(II) and Zn(II) in the range 0.01–0.25 mg L 1. The method was applied successfully in water analysis.  相似文献   

10.
We have developed a laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) method to directly determine the concentrations of trace metals in high-purity powdery silicon carbide (SiC) samples. The sample preparation procedure is simple and rapid. The sample was formed into pellets using no binders and heated at 1000 °C for 2 h. The operation parameters for LA and ICP-MS were optimized to achieve a table signal intensity and high sensitivity. National Institute of Standards and Technology Standard Reference Materials glasses were chosen as calibration standards, with 29Si chosen as the internal standard. The relative sensitivity factor obtained from the glass matrix was used to calculate the concentrations of analytes in the SiC ceramic samples. The regression correlation coefficients of the calibration curves for elements with internal standard correction ranged from 0.9981 to 0.9999, which are better than those obtained with an external standard correction method only. The relative standard deviation of the measured trace element concentrations was less than 5%. The limits of detection were 0.02, 0.08, 0.04, 0.005, 0.01, 0.02, 0.004, 0.07, and 0.006 mg kg 1 for B, Ti, Cr, Mn, Fe, Ni, Co, Cu, and Sr, respectively. The method was applied to analyze SiC samples with two different particle sizes. The analysis showed good agreement with the results of inductively coupled plasma optical emission spectrometry. The reliability of the proposed method was confirmed by determining the contents of B, Ti, Cr, Mn, Fe, Ni, and Cu in BAM-S003.  相似文献   

11.
An automated solid phase extraction method by flow analysis on-line inductively coupled plasma mass spectrometry (FI-ICP-MS) for the determination of cobalt, chromium, nickel, cadmium, manganese, zinc, copper and lead in sea-water and other natural waters is described. The system is based on retention of the analytes onto a minicolumn packed with a chelating resin, 1,5-bis (2-pyridyl)-3-sulphophenyl methylene thiocarbonohydrazide immobilized on aminopropyl-controlled pore glass, placed in the injection valve of a simple flow manifold. The effects of chemical and flow variables were investigated and selected as a compromise between sensitivity and sampling frequency. So, the sample solutions (adjusted to pH 8.0 ± 0.5) were passed through the column. After washing the column with water, the adsorbed metals were subsequently eluted into the plasma with 4% m/m nitric acid. Detection limits of the trace metals (180 s sample loading time at a sample flow rate of 0.7 mL min? 1; sampling frequency 8.6 h? 1) were 0.002 μg L? 1 for Co, 0.057 μg L? 1 for Cr, 0.117 μg L? 1 for Ni, 0.004 μg L? 1 for Cd, 0.210 μg L? 1 for Mn, 0.260 μg L? 1 for Zn, 0.030 μg L? 1 for Cu and 0.020 μg L? 1 for Pb, with enrichment factors between 2.2 and 6.8. The accuracy of the proposed method was checked with certified reference materials (CRMs) of sea-water SLEW 3, LGC6016 and CASS-5, river water SLRS-5 and fortified lake water TMDA-54.4. The results from the determination of these metals were in agreement with the certified values and recovery values ranged between 92.2 and 110.6%. The method was applied to the determination of these metal ions in sea-water samples collected in the Málaga Bay in order to realize a pilot study necessary to generate preliminary information on which to base a more detailed pollution study by heavy metals of the Bay.  相似文献   

12.
Here we reported that UV light irradiation can significantly enhance sensitivity of Ti/TiO2 electrode for determination of trace heavy metal ions (such as Cu2 +, Pb2 + and Cd2 +) owing to the photodeposition of metal ions on the surface of electrodes. The sensitivity of heavy metal ions can be selectively enhanced over the Ti/TiO2 electrode, which is attributed to matching between potential of heavy metal ions and the position of the conduction band of TiO2.  相似文献   

13.
The present research was conducted to study heavy metal contamination in roadside soil viz. (i) at sites having more than two traffic signals (ii) roads having only one traffic signal and (iii) roads having no traffic signals. The samples were collected and analyzed for seven heavy metals i.e. cadmium (Cd), lead (Pb), copper (Cu), nickel (Ni), iron (Fe), manganese (Mn) and zinc (Zn) by Atomic Absorption Spectroscopy (AAS) following the acid digestion of the respective soil samples. The range of the metals observed in soil having more than two traffic signals were Cd (0.17–1.01), Pb (259.66–2784.45), Cu (15.51–65.90), Ni (13.31–98.13), Fe (325.64–5136.37), Mn (57.95–166.43), and Zn (91.34–166.43) mg kg?1 respectively. Similarly, the range of metals analyzed in samples collected from the roadside having only one traffic signal were Cd (nd–0.80), Pb (145.95–308.09), Cu (0.82–18.04), Ni (18.29–59.36), Fe (88.51–3649.42), Mn (25.88–147.34) and Zn (8.97–106.11 mg kg ?1) respectively. However, the range of metals at roads having no traffic signals were Cd (0.0–0.57), Pb (8.34–58.20), Cu (2.88–5.81), Ni (3.34–73.80), Fe (55.34–332.81), Mn (2.98–98.73) and Zn (1.23–46.6 mg kg?1) respectively. Cd, Cu, Ni, Fe, Mn and Zn in soil were present within the normal range of background levels, whereas lead was reported in high concentration. The level of lead had a correlation with the traffic density attributing its origin to vehicular exhaust. The values from three different sites of monitoring suggest that automobiles are a major source of the studied metals for the roadside environment.  相似文献   

14.
This paper represents the first work on the concentrations of heavy elements, physiochemical characteristics and activity levels of the naturally occurring radionuclides in the Saudi Arabian coastline of the Gulf of Aqaba. Concentrations of 19 heavy elements were measured, namely: Ag, Al, As, Ba, Be, Cd, Co, Cr, Cu, Fe, Hg, Mn, Mo, Ni, Pb, Sb, Se, V and Zn. The radioactivity levels of 238U, 232Th and 40K were estimated to be: 17 ± 1.7, 22.5 ± 3.7 and 649.6 ± 64.2 Bq kg?1, respectively. The measurements were carried out using inductively coupled plasma-mass spectrometry (ICP-MS). In addition, physiochemical characteristics of 19 sediment samples (i.e., saturation percentage, pH, electrical conductivity, organic matter, cation exchange capacity and content of clay, silt and sand) have been determined. Indications for high correlation between most heavy elements are found. The correlation between heavy elements and the radionuclides 238U, 232Th and 40K was generally significant.  相似文献   

15.
Cu was determined in a wide range of petroleum products from crude oil distillation using flame atomic absorption spectrometry (FAAS), electrothermal atomic absorption spectrometry (ETAAS) and inductively coupled plasma mass spectrometry (ICP-MS). Different procedures of sample preparation were evaluated: (i) mineralization with sulfuric acid in an open system, (ii) mineralization in a closed microwave system, (iii) combustion in hydrogen–oxygen flame in the Wickbold's apparatus, (iv) matrix evaporation followed by acid dissolution, and (v) acidic extraction. All the above procedures led to the transfer of the analyte into an aqueous solution for the analytical measurement step. It was found that application of FAAS was limited to the analysis of the heaviest petroleum products of high Cu content. In ICP-MS, the use of internal reference method (with Rh or In as internal reference element) was required to eliminate the matrix effects in the analysis of extracts and the concentrated solutions of mineralized heavy petroleum products. The detection limits (in original samples) were equal to, respectively, 10, 86, 3.3, 0.9 and 0.4 ng g 1 in procedures i–v with ETAAS detection and 10, 78, 1.1 and 0.5 ng g 1 in procedures i–iii and v with ICP-MS detection. The procedures recommended here were validated by recovery experiments, certified reference materials analysis and comparison of results, obtained for a given sample, in different ways. The Cu content in the analyzed samples was: 50–110 ng g 1 in crude oil, < 0.4–6 ng g 1 in gasoline, < 0.5–2 ng g 1 in atmospheric oil, < 6–100 ng g 1 in heavy vacuum oil and 140–300 ng g 1 in distillation residue.  相似文献   

16.
A galvanostatic anodization is used to prepare long TiO2 nanotube arrays (TNTAs). TNTAs of over 100 μm in length, with similar nanotube size and structural regularity to the classic TNTAs made from potentiostatic mode, are achieved at 10 mA cm 2. After a post-anodization in a H3PO4-based electrolyte, the TNTAs with long nanotubes exhibit good adhesion to Ti substrate. The as-prepared long TNTAs yield a larger areal capacitance of 128.4 mF cm 2. Further, the long TNTAs possess a higher surface area, making them suitable as support templates for other active materials.  相似文献   

17.
Multi-walled carbon nanotubes (MWCNTs) were used successfully for the removal of heavy metals from aqueous solution. Characterization techniques showed the carbon as nanotubes with an average diameter between 40 and 60 nm and a specific surface area of 61.5 m2 g?1. The effect of carbon nanotubes mass, contact time, metal ions concentration, solution pH, and ionic strength on the adsorption of Cu(II), Pb(II), Cd(II) and Zn(II) by MWCNTs were studied and optimized. The adsorption of the heavy metals from aqueous solution by MWCNTs was studied kinetically using different kinetic models. A pseudo-second order model and the Elovich model were found to be in good agreement with the experimental data. The mechanism of adsorption was studied by the intra-particle diffusion model, and the results showed that intra-particle diffusion was not the slowest of the rate processes that determined the overall order. This model also revealed that the interaction of the metal ions with the MWCNTs surface might have been the most significant rate process. There was a competition among the metal ions for binding of the active sites present on the MWCNTs surface with affinity in the following order: Cu(II) > Zn(II) > Pb(II) > Cd(II).  相似文献   

18.
The determination of chromium (VI) compounds in plants by electrothermal atomic absorption spectrometry (ET AAS) is proposed based on their leaching with 0.1 M Na2CO3. Due to the presence of relatively high amounts of Na2CO3 in the resulting samples, the temperature and time of pyrolysis and atomization stages must be optimized to minimize the influence of the matrix. A limit of detection (LOD) for determination of Cr(VI) in plants by ET AAS was found to be 0.024 μg g−1.The concentration of Cr(VI) and total chromium in plants collected in different geographical areas (South Africa and Russia), grown on soils high in chromium was determined. The concentration of Cr(VI) and total Cr in stems and leaves of plants was in the range of 0.04–0.7 μg g−1 and 0.5–10 μg g−1, respectively. The limited uptake of Cr(III) by plants, in comparison to its concentration in soil, can be explained by the very low solubility of natural Cr(III) compounds.Results for the determination of Cr(VI) were confirmed by the analysis of BCR CRM 545 (Cr(VI) in welding dust) with good agreement between certified (39.5 ± 1.3 μg mg−1) and found (38.8 ± 1.2 μg mg−1) values. The total concentration of Cr in plants has also been determined by ET AAS after dry ashing of samples at 650 °C. Results were confirmed by the analysis of BCR CRM 281 (Trace elements in Rye Grass) with good agreement between the found (2.12 ± 0.16 μg g−1) and certified value (2.14 ± 0.12 μg g−1).  相似文献   

19.
《Comptes Rendus Chimie》2015,18(10):1007-1012
Cordierite-supported structured catalysts were prepared with several alumina-based suspensions containing K, Cs or Ba as alkali promoter, and Co, or Cu as active metals. The prepared catalysts were tested in a lab installation with a gas hourly space velocity (GHSV) from 1300 h−1 to the one representative of the exhaust gases of a diesel engine, i.e. GHSV = 36,690 h−1. Significant differences in the behavior of the catalysts are observed when increasing the GHSV, pointing to different predominant factors taking place in each case depending on the active metal and the alkali promoter used.  相似文献   

20.
A Re coil-filament in-torch vaporization (ITV) sample introduction system was interfaced to a sector field inductively coupled plasma-mass spectrometry (SFICP-MS) system. In this first report on an un-optimized ITV-SF-ICP-MS system, detection limits were established using 5 μL volumes of 100 pg mL 1 standard solutions, translating to 0.5 pg absolute. Such absolute amounts of a dried solution are near or below the detection limit of many ICP-based techniques. The absolute detection limits for Cd, Eu, Pb, Ti, U and Zn were in the 0.2–2 fg range (or, in the 10's of millions to millions of atoms for Pb, Cd, Zn and Ti, about one million atoms for U and about 800 thousand for Eu). These absolute detection limits along with the ability of ITV to handle minute amounts of discrete samples (thus eliminating memory effects from nanoparticles adhering to the walls of pneumatic nebulization sample introduction systems and from clogging of the mass spectrometer orifice), use of sonicated water-based slurries (that eliminated contamination from acid digestion reagents or from slurry stabilization reagents), and elimination of oxygen containing molecular ion interferences due to use of dry samples enabled concentration determinations of Ti (and consequently of TiO2) in pg mL 1 concentrations of slurries of manufactured, 20 nm diameter TiO2 nanoparticles.  相似文献   

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